Combining Raman Microprobe and XPS to Study High Temperature Oxidation of Metals

Raman microprobe spectroscopy was applied in studies of high-temperature air oxidation of a ferritic alloy (HT-9) in the absence and presence of zirconia coatings with the objective of evaluating the technique as a way to quickly screen candidate cladding materials and actinide-based mixed oxide fuel mixtures for advanced nuclear reactors. When oxidation was relatively uniform, Raman spectra collected using microscope optics with low spatial resolution were found to be similar to those collected with conventional Raman spectroscopy. These spectra could be used to identify major oxide corrosion products and follow changes in the composition of the oxides due to heating. However, when the oxidation films were comprised of multiple layers of varying composition, or with layers containing metallic phases, techniques with higher depth resolution and sensitivity to zero-valence metals were necessary. The requirements were met by combining Raman microprobe using different optical configurations and x-ray photoelectron spectroscopy.